CN103897796A - Method for extracting blueberry seed oil by adopting ultrasonic-assisted aqueous enzymatic method - Google Patents
Method for extracting blueberry seed oil by adopting ultrasonic-assisted aqueous enzymatic method Download PDFInfo
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Abstract
The invention discloses a method for extracting blueberry seed oil by adopting an ultrasonic-assisted aqueous enzymatic method. The method for extracting the blueberry seed oil by adopting the ultrasonic-assisted aqueous enzymatic method comprises the following steps: carrying out breaking, pulverization and then enzymolysis treatment on blueberry seed taken as raw material, applying certain ultrasonic for assisting extraction in different stages, then carrying out enzyme deactivation and centrifugation, and taking a supernate, so that the blueberry seed oil is obtained. The method for extracting the blueberry seed oil is simple in operation, mild in conditions, high in oil yield, pollution-free, easy for refining, low in production cost and applicable to large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method of edible oil, especially relate to a kind of method that ultrasonic wave auxiliary water enzyme process is prepared blueberry seed oil.
Background technology
Blueberry, claims again cowberry, blue berry, is Ericaceae genus vaccinium plant, is perennial fallen leaves or evergreen shrubs.Blueberry is berry, and subcircular is blue, moderately sour and sweet, and pulp exquisiteness, the thin seed of skin is little.Blueberry is rich in abundant nutritive ingredient, comprises the materials such as anthocyanidin, VitAVitE, ursolic acid, ellagic acid and polyphenol, has the effects such as the eyesight of raising, anti-ageing, cardiac function enhancing, Cardiovarscular and reduction cholesterol.Therefore, blueberry in recent years fashionable both at home and abroad, classified as by Britain authority nutritionist and Food and Argriculture OrganizationFAO respectively " 15 kinds of heath food " first of and one of " the large heath food of the mankind five ".
Blueberry seed is the by product of the converted productss such as blueberry juice, fruit wine and snackfoods.Blueberry seed oil is rich in the unsaturated fatty acids of higher proportion, and wherein contained alpha-linolenic acid is the polyene unsaturated fatty acid of n-3 series, and metabolism is EPA and DHA in vivo, and it is special on biomembranous structure and function, to play a part.Long-term edible blueberry seed oil can effectively reduce cholesterol level, and vision protection, increases intelligence, the preventive and therapeutic effect positive to having of the disease such as cardiovascular and cerebrovascular and cancer.Meanwhile, blueberry seed oil contains abundant vitamin-E, has anti-oxidation efficacy, and the cytolemma of protection skin, can reduce UV-induced skin lesion; Its still a kind of good crease-resistant oil, can effectively releive tiny wrinkle and cell tissue regeneration, the elasticity of maintenance skin, prevents skin aging.Therefore, exploitation blueberry seed oil, not only for Vegetable oil lipoprotein and Cosmetic Market provide as new function grease, meet human consumer's different demands, and can also make full use of blueberry industry processing byproduct, and reduce environmental pollution, there is considerable Social benefit and economic benefit.
Grease extracts main milling process, organic solvent extractionprocess and the supercritical extraction etc. of adopting both at home and abroad.Wherein considerably less about the report of the extraction of blueberry seed oil, utilize ultrasonic wave secondary solvent extraction process (Chen Liang etc., the research of blueberry seed oil component, Chinese oil, 2013, 38:10, 84-86.), the method is to utilize blueberry seed oil difference of solubleness in different solvents to extract blueberry seed oil, technique is comparatively simple, the oil yield of its blueberry seed oil is in 18% left and right, but it need to carry out repeatedly lixiviate repeatedly for a long time to blueberry seed oil, exist blueberry seed oil crude oil color and luster dark, the problems such as residual solvent is more, affect to a certain extent the fragrance of blueberry seed oil, and in heat-processed, make solvent evaporates cause environmental pollution, utilize in addition in addition relevant report (the Qu little Yuan etc. of supercritical fluid extraction blueberry seed oil, blueberry seed oil analysis of volatile components, Guizhou Agricultural Sciences, 2013,41:10,64～66), this method is to control blueberry seed oil solubleness and vapor partial pressure therein by the pressure and temperature of adjusting CO2 to extract blueberry seed oil, and without the need for machine solvent, but its oil yield to blueberry seed oil only has 8% left and right, and required equipment is more expensive, be not suitable for suitability for industrialized production.
Summary of the invention
Object of the present invention is exactly the above-mentioned shortcoming existing for prior art, a kind of method of ultrasonic wave auxiliary water Enzymatic Extraction blueberry seed oil is provided, and blueberry seed that the method obtains oil oil yield is high, quality of crude oil is high, organic solvent-free is residual, be easy to realize industrial applications.
The object of the invention is to realize in the following manner:
It is 60～80 object blueberry seed powder that the pulverizing of blueberry seed is obtained to particle diameter, and water is mixed with blueberry seed powder suspension, under 40～60 ℃ of conditions, is incubated, ultrasonication 10～20min, supersound process power is 300～500W, and preferably treatment power is 400W, adds proteolytic enzyme and the Mierocrystalline cellulose-pectin compound enzyme of blueberry seed opaque amount 1.0～3.5%, ultrasonic assistance enzymolysis 20～40min, ultrasonic power is 60～90W, and preferably ultrasonic power is 90W, and enzyme goes out, centrifugal, collect supernatant liquor and get final product.
In described blueberry seed powder suspension, the mass ratio of blueberry seed powder and water is 1:3～1:8.Commercially available blueberry seed raw material all can use.Raw material blueberry seed water content can be controlled to 8%～10%.
The proteolytic enzyme of selecting and Mierocrystalline cellulose-pectin compound enzyme are all acidicenzyms, and the weight ratio of proteolytic enzyme and Mierocrystalline cellulose-pectin compound enzyme is 1:1～1:3.
Above-mentioned ultrasonication and ultrasonic assistance enzymolysis are processed preferably and are bathed under heat-retaining condition and carry out at 40～50 ℃ of Water Unders.
The mode that the enzyme that goes out adopts can adopt 100 ℃ of Water Unders to bathe and process 10min.
Described centrifugal condition is rotating speed centrifugal 20～30min under 10000r/min condition.
The extracting method that the present invention specifically takes is as follows: blueberry seed is added and in pulverizer, pulverizes 30s, cross 60～80 mesh standard sieves and obtain blueberry seed powder, blueberry seed powder and tap water are mixed with the blueberry seed powder suspension that mass ratio is 1:3～1:8, bath temperature is set 40～60 ℃ of insulations, at this temperature, ultrasonication 10～20min, ultrasonic power is 300～500W, add proteolytic enzyme and the Mierocrystalline cellulose-pectin compound enzyme of blueberry seed opaque amount 1.0～3.5%, wherein, the weight ratio of proteolytic enzyme and Mierocrystalline cellulose-pectin compound enzyme is 1:1～1:3, after stirring, reduce ultrasonic power to 60～90W, ultrasonic assistance enzymolysis 20～40min under 40～60 ℃ of conditions, warming-in-water to 100 ℃ more afterwards, boiling water bath 10min goes out after enzyme, centrifugal 20～30min under 10000r/min speed conditions, collect supernatant liquor and get final product.
Blueberry seed oil fatty acid quality and constitutes analysis method are as follows:
(1) esterification processing: accurately take blueberry seed oil 0.3g and be placed in 10mL scale sample bottle, add successively 5mL normal hexane, 3mL0.05% potassium hydroxide-methanol solution, be placed in 60 ℃ of water-baths and react 30min, be settled to 10mL with distilled water, vibration evenly, the centrifugal 5min of 10000r/min, gets supernatant liquor and carries out gas chromatographic analysis.
(2) chromatography of gases analysis: Agilen6890 chromatographic instrument, (30m × 0.32mm × 0.25 μ m) for HP-5 quartz capillary column, carrier gas is N2, and flow is 1mL/min, and detector is FID, sample size is 1 μ L, splitting ratio is 40:1, and injection port and detector temperature are respectively 260 ℃ and 280 ℃, temperature programming: 150 ℃ of maintenance 5min of initial temperature, rise to 250 ℃ with 10 ℃/min, keep 10min.
The present invention is in blueberry seed cracking process, and apply high-power ultrasonics direct effect blueberry seed powder suspension early stage, transfers afterwards low frequency ultrasound assistance enzymolysis to.Hyperacoustic extraction strengthening effect is to be mainly powerful shockwave and the micro-acoustic streaming producing in moment due to cavitation effect, destroys cell wall structure its content is fully discharged.But hyperacoustic excessive use also can produce some adverse consequencess, as accelerated Oxidation of Fat and Oils, produce metallic, rancid smell, also can produce detrimentally affect to the lipid acid composition of grease to a certain extent simultaneously.In addition, the impact of ultrasonic wave on enzyme reaction, under different conditions, result is very different.If the ultrasonic power adopting when enzyme reaction is excessive, will cause enzyme deactivation; Lower powered ultrasonic wave has played positive katalysis to enzyme reaction.
Contriver further illustrates hyperacoustic operation parameter in leaching process by following test after by a large amount of preliminary experiments again, and with the synergy of enzymolysis:
1) impact of ultrasonic pretreatment on seed oil oil yield and oil quality:
Bathe the blueberry seed powder suspension (weight ratio that is 60-80 order blueberry seed powder and tap water is 1:4) of insulation to 40～60 ℃ of Water Unders, the different Ultrasonic Conditions that apply respectively 200～600W carry out extraction process 15min, measure its blueberry seed powder oil yield and unsaturated fatty acids wherein (being the acid of blueberry seed oil fatty) ratio, the crude oil extracting is carried out to sensory evaluation, test result is as table 1 simultaneously:
Table 1
| Ultrasonic power/W | Ultrasonic time/min | Oil yield/% | Grease organoleptic quality | Unsaturated fatty acids ratio % |
| 200 | 15 | 12.45 | Free from extraneous odour | 85.78 |
| 300 | 15 | 13.85 | Free from extraneous odour | 92.76 |
| 400 | 15 | 15.42 | Free from extraneous odour | 90.22 |
| 500 | 15 | 17.55 | Slight rotten odor | 90.25 |
| 600 | 15 | 18.55 | Obviously metallicity, rotten odor | 89.45 |
2) effect of ultrasound-assisted enzymolysis effect:
Get 40～60 ℃ of Water Unders and bathe the blueberry seed powder suspension (weight ratio that is 60-80 order blueberry seed powder and tap water is 1:4) of insulation, after 400W supersound process 15min, under these 40～60 ℃ and 400W ultrasound condition, add a certain proportion of proteolytic enzyme and pectin-cellulose complex enzyme (mass ratio of proteolytic enzyme and pectin-cellulose complex enzyme is 1:1), reduce power to below shown in form, ultrasonic assistance enzymolysis 30min, all the other steps are with embodiment 1, measure blueberry seed oil yield, test result is as table 2:
Table 2
| Assisting ultrasonic power/W | Enzymolysis time/min | Enzyme concentration | Oil yield/% |
| 0 | 30 | 3.5% | 18.22 |
| 30 | 30 | 3.5% | 20.35 |
| 60 | 30 | 2.5% | 24.62 |
| 90 | 30 | 2.5% | 25.55 |
| 120 | 30 | 2.5% | 21.44 |
| 150 | 30 | 2.5% | 17.54 |
Consider the impact of ultrasonic wave on oil yield and oil quality, preferably ultrasonication power is 300～500W, and most preferably ultrasonication power is 400W, and the preferred power of later stage low power ultrasound assistance enzymolysis is 60～90W, most preferably 90W.
The invention has the beneficial effects as follows compared with the prior art:
1) according to method provided by the invention, blueberry seed oil oil yield high (all more than 24%), quality of crude oil is high, and organic solvent-free is residual, and wherein unsaturated fatty acids ratio is up to more than 90%
2) compared with prior art, guaranteeing under the prerequisite of oil yield, by ultrasonic and associated treatment enzymolysis; extraction conditions gentleness, had both alleviated the detrimentally affect of ultrasonic wave to oil quality, had at utmost protected the quality of crude oil; the usage quantity of simultaneously saving enzyme, has reduced cost.
Embodiment
In order to understand more clearly the present invention, below in conjunction with example, the present invention is described further.But the detail of embodiment only, for explaining the present invention, does not limit the present invention in any way.
Embodiment 1:
By blueberry seed (water content is 8%), being ground into particle diameter is 60 object blueberry seed powder.Take the blueberry seed powder 10g after pulverizing, be mixed with blueberry seed powder suspension with tap water, the mass ratio of blueberry seed powder and water is 1:3, bath temperature is set in 40 ℃, ultrasonication 15min, ultrasonic power is 400W, add successively the proteolytic enzyme (purchased from Nanjing Olympic Duo Fu Buddhist nun bio tech ltd) of blueberry seed opaque amount 1.25% and the Mierocrystalline cellulose-pectin compound enzyme (purchased from Nanjing Olympic Duo Fu Buddhist nun bio tech ltd) of blueberry seed opaque amount 1.25%, after stirring, reduce ultrasonic power to 90W, ultrasonic assistance enzymolysis 30min, improve again bath temperature to 100 ℃, boiling water bath goes out after enzyme 10mim, adopt high speed freezing centrifuge, centrifugal 25min under 10000r/min speed conditions, collect supernatant liquor and obtain yellow bright blueberry seed oil.The method blueberry seed oil yield is 25.82%, and in the blueberry seed oil obtaining, unsaturated fatty acid content is 92.15%.
Embodiment 2:
To obtain blueberry seed (water content is 9%), being ground into particle diameter is 60 object blueberry seed powder.Take the blueberry seed powder 50g after pulverizing, be mixed with blueberry seed powder suspension with tap water, the mass ratio of blueberry seed powder and water is 1:6, bath temperature is set in 60 ℃, ultrasonication 20min, ultrasonic power is 300W, add successively the proteolytic enzyme of blueberry seed opaque amount 0.5% and the Mierocrystalline cellulose-pectin compound enzyme of blueberry seed opaque amount 1%, after stirring, reduce ultrasonic power to 90W, ultrasonic assistance enzymolysis 20min, improve again bath temperature to 100 ℃, boiling water bath is processed 10min and is gone out after enzyme, adopt high speed freezing centrifuge, centrifugal 30min under 10000r/min speed conditions, collect supernatant liquor, obtain yellow bright blueberry seed oil.The method blueberry seed oil yield is 24.55%, and in the blueberry seed oil obtaining, unsaturated fatty acid content is 91.85%.
Embodiment 3:
By blueberry seed (water content is 10%), being ground into particle diameter is 80 object blueberry seed powder.Take the blueberry seed powder 100g after pulverizing, be mixed with blueberry seed powder suspension with tap water, the mass ratio of blueberry seed powder and water is 1:8, water bath heat preservation is set in 50 ℃, ultrasonication 10min, ultrasonic power is 500W, add successively the proteolytic enzyme of blueberry seed opaque amount 0.8%, Mierocrystalline cellulose-the pectin compound enzyme of blueberry seed opaque amount 2.4%, after stirring, reduce ultrasonic power to 75W, ultrasonic assistance enzymolysis 40min, improve again bath temperature to 100 ℃, boiling water bath is processed the 10min enzyme that goes out, adopt high speed freezing centrifuge, rotating speed is centrifugal 20min under 10000r/min condition, collect supernatant liquor, obtain yellow bright blueberry seed oil.The method blueberry seed oil yield is 26.18%, and in the blueberry seed oil obtaining, unsaturated fatty acid content is 90.45%.
Claims (9)
1. the method for ultrasonic wave auxiliary water Enzymatic Extraction blueberry seed oil, is characterized in that the method comprises the following steps:
It is 60～80 object blueberry seed powder that the pulverizing of blueberry seed is obtained to particle diameter, water is mixed with blueberry seed powder suspension, under 40～60 ℃ of conditions, be incubated, ultrasonication 10～20min, processing power is 300～500W, add proteolytic enzyme and the Mierocrystalline cellulose-pectin compound enzyme of blueberry seed opaque amount 1.0～3.5%, ultrasonic assistance enzymolysis 20～40min, ultrasonic power is 60～90W, enzyme goes out, centrifugal, collect supernatant liquor and get final product.
2. the method for utilizing ultrasonic wave auxiliary water Enzymatic Extraction blueberry seed oil according to claim 1, is characterized in that: in described blueberry seed powder suspension, the mass ratio of blueberry seed powder and water is 1:3～1:8.
3. the method for utilizing ultrasonic wave auxiliary water Enzymatic Extraction blueberry seed oil according to claim 1, is characterized in that: the consumption weight ratio of described proteolytic enzyme and Mierocrystalline cellulose-pectin compound enzyme is 1:1～1:3.
4. the method for utilizing ultrasonic wave auxiliary water Enzymatic Extraction blueberry seed oil according to claim 1, is characterized in that: ultrasonication and ultrasonic assistance enzymolysis are processed at 40～50 ℃ of Water Unders and bathed under heat-retaining condition and carry out.
5. the method for utilizing ultrasonic wave auxiliary water Enzymatic Extraction blueberry seed oil according to claim 1, is characterized in that: the mode that the enzyme that goes out adopts is that 100 ℃ of Water Unders are bathed processing 10min.
6. the method for utilizing ultrasonic wave auxiliary water Enzymatic Extraction blueberry seed oil according to claim 1, is characterized in that: described centrifugal condition is rotating speed centrifugal 20～30min under 10000r/min condition.
7. the method for utilizing ultrasonic wave auxiliary water Enzymatic Extraction blueberry seed oil according to claim 1, is characterized in that: described blueberry seed water content is 8%～10%.
8. the method for utilizing ultrasonic wave auxiliary water Enzymatic Extraction blueberry seed oil according to claim 1, is characterized in that: described pre-treatment power is 400W.
9. the method for utilizing ultrasonic wave auxiliary water Enzymatic Extraction blueberry seed oil according to claim 1, is characterized in that: the power that described ultrasonic assistance enzymolysis uses is 90W.
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